Antifelting of wool



Patented July 18, 1950 UNITED STATES PATENT OFFICE ANTIFELTING ,OF WOOL Frederick E. Haigh, Passaic, Hugo Ehrhardt, Nutley, and Ernest C. Koerner, Belvidere, N. J., assignors to Botany Worsted Mills, a corporation of New Jersey No Drawing. Application April 1, 1947,

Serial No. 738;724

Claims. (01. 8-4155) rials retain their color without significant impairment, if they have been dyed prior to the application of the resin. Furthermore, it has been found that there is an improvement in the color tone and depth in many cases.

As an example, 100% wool flannel fabric was subjected to a chlorinating bath prepared according to usual practice from commercial hypochlorite, suitably acidified and adjusted. When the fabric was subjected to the bath, the bath was suitably replenished and maintained con- It has long been sought to provide an effective process for anti-felting wool. Various methods have been proposed, such as chlorination, or resin treatment, or treatment of the wool with alkali, treatment of the textiles with alkaline alcoholic solutions, the subsequent treatment of alkali treated wool with a pre-polymerized resin, or a non-polymerized resin. In such latter cases, the method is completed by polymerizing the resin by the use of heat or other means after its application to the textiles. In all these processes there are objections which lie in the impairment of the wool product as to hand and tensile strength, incomplete anti-felting, inefficient antifelting, change in color of the dyed wool fabrics, destruction of the wool by impairment in the treating bath, by moisture brought into the bath by the wool itself, etc., etc. This latter impairment has been found to exist in the employment of a proposed alkaline, causticsynthetic resin treatment, wherein the caustic is in an alcoholic solution. In this process, one furthermore receives a stiff, boardy, tacky and stick hand. If the textiles have been dyed prior to resin treatment, many shades and usually the more commercially favored shades such as bright'anol pastel shades are altered materially by the efiect of the resin treatment. If the materials are to be dyed'they will frequently not accept color subsequent to the resin treatment or their nonfelting propertie obtained during the resin treatment are substantially impaired or lost in the subsequent dyeing bath. v

' The characteristic feature of our process is a combination of a patrial halogenation of the wool followed by application to the wool of a resin such as polymerized olefins suitably dispersed and stabilized in an aqueous medium. The resinsolution tends to confine the wool pick up of the resin to the outer structure oflthe'fiber itself without apparently filling the normally hollow core'of the fiber. This maybe the cause for the highly desirable, soft hand which is present after the treatment has been completed. Our method, is such that normally dyed matee stantly at theoretically between 0.03% and 0.05% free chlorine. Actually'it was somewhat less due to evaporation.

The flannel was thereafterdechlorinated with sodium bisulphite in the customary manner.

Thereafter the flannel was rinsed in cold water and then dried The flannel fabric was then tested for shrinkage and the result wasshown as follows:

Table 1 [Shrinkageof flannel after 18 washings. 3 (All washings referred to according to COO-T-lQl-a, Federal Specifications for Textiles, April 23, 1937.)]

Untreated Chlorinated Flannel, Flannel, Warp Warp Percent Percent 41. 6 26. 3

Table 2 [After 18 washings: conditions as before stated: shrinkage] H The resin treatment alone is unsatisfactory because the fabric is rendered sticky, tacky, and boardy, and furthermore showed a considerable change in appearance and color. It can therefore be stated that the resin treatment alone is unsatisfactory as it leaves the fabric commercially undesirable.

It will be noticed furthermore that the chlorination treatment alone leaves the fabric subject to high shrinkage.

Our next step was to pad another sample of partially chlorinated 100% wool flannel fabric with a polymerized olefin resin, a suitable commercial product for this purpose being sold under the trade name Durlana by the Warwick Chemical Division of the Sun Chemical Go, West Warwick, R. I. 25% solids was mixed with 0.3 liter of a suitable wetting agent, such as the sulphonated oil (sulfonol R manufactured by the Warwick Chemical Division of the Sun Chemical Co. being [After l8.washii1gs: conditions as before stated: shrinkage] Partially Chlorln- $5353.51 annel with. W olid Durlana up onflber, Warp Percent Percent 41. 6 3 1 As. is well known,v if the chlorination process alone is used to reach the non-felting point, the end product of such a chlorination process cannot be dyed commercially, its tensile strength is substantially impaired, its hand. is substantially depreciated, it is harsh, and the wearability of the textile product is considerably deteriorated. When a product is halogenated to the non-felting point, it is not truly washable, tending to disintegrate rapidly upon washing and showing a substantial weight loss. The product will even extend in size because of fiber slippage.

On the other hand, in order to obtain nonfelting properties by the use of resins alone, amounts of foreign matter exceeding the allowance of the wool label act are required, the product is stiff and boardy, sometimes sticky, especially on ageing, altered in shade if. dyed, and cannot be dyed to commercial levelness of shade if treated undyed and then dyed.

In our process we do not complete the halogenation up to the. non-felting point and we furthermore do not use amounts of resins exceeding the allowance for foreign matter made in the wool labelling act.

In our process we can halogenate and dye without the deleterious effects of damaging the color and without impairing the tensile strength but rather improving the tensile strength of the original product. Our process allows to either halogenate and dye thereafter, or to dye and halogenate thereafter. The material after our halogenation process is not at the non-felting point. The non-felting point is reached through our halogenation process together with a resin treatment. We can also dye after the dual process is completed, i. e., after the halogenation and the resin treatment. This is due to the mild halogen concentration in the bath 16 liters of the resin solution containing and the small amounts of resin deposited on the surface of the fabric wherein the resin does not act as a resisting surface, due to its slight concentration upon the textile surface. It. is to be noted that the halogenation in this process is stopped at a point where the tensile strength of the fabric has not been impaired. In fact, we find that our halogenation procedure tends to increase the tensile strength of fabrics slightly. This can be explained as follows: The halogenation process slightly gelatinizes the surface of the fibers; upon halogenat'ion the adjacent surfaces tend to fuse slightly, thus reducing the slippage of the fibers and resulting, in a satisfactory fabric of great strength. If. a. dyed fabric is halogenated to the extent of making. itnon-felting, the color is impaired beyond the point of commercial acceptance. On the other hand, if an undyed fabric is so treated, it cannot then be d'yed to commercial levelness of shade. A similar condition exists with resin treatments. If a dyed fabric is treated with a resin to a sufiicient extent to render it non-felting, most colors are altered beyond the point of commercial acceptanceor if the fabric so treated is notyet dyed, then the subsequent dyeing can not be done to a, commercial degree of levelness and it also usually materially reduces the non-felting properties previously obtained. In this new process these difiiculties do not arise as both the halogenation and the after treatment with resin are such that colors are not altered beyond the point of commercial acceptance. In fact, we have definitely established that we can dye, halogenate, and resin treat or halogenate, dye and resin treat, and finally halogenate and resin treat and thereafter dye, obtaining pure shades of any color by means of all three techniques without impairing the result of our previous anti-felting treatment. The specific feature in this new process resides in the fact that it is possible to make the dyeing the final step of the process. This permits very exact shade control and exact shading control yields to very satisfactory color matching.

Our process comprises two steps which can be combined and interchanged variably with the other customary procedures for the treatment of textiles, such as laking and dyeing. Our process consists of the first step, of a partial halogenation of the textiles, and of the second step, a special resin treatment of the. partially halogenated textiles.

After plain. wetting in water, the goods are immersed. for a period of approximately seconds at ambient temperture in a solution containing from 0.03% to 0.09% of acidified solution. After immersion, the textile material is dechlorinated in the customary manner with a weak solution of sodium bisulphite. The goods are rinsed and then hydro-extracted in a con ventional hydro-extractor and dried. The dried goods are then impregnated with a resin solution in the customary manner. The amount of resins used are very small as explained elsewhere in this. application. The resin treated goods are then dried or cured. Under certain conditions the goods may then be given a mild washing to remove excess resin particles. In the course of this washing or subsequent thereto, softening agents may be applied to produce a very soft handling effect. Thereafter the goods are dried again and are now ready for use or may be subjected to the usual wool textile finishing operations, such as. but not restricted to.

napping, shearing, pressing, decating, etc. The above procedure is given by way of exemplification, but is not intended to limit the scope of the invention described herein.

.For the purpose of resin treatment applied to our partially halogenated wool product the following resins have been found satisfactory: Poly-a merized di-olefines such as Durlana by the Warwick Chemical Division of the Sun Chemical Go, West Warwick, R. I., Koloc resins 'm ariuw. factured and commercially sold by the U. S. Rubber Company of Passaic, New Jersey, melamine and melamine-formaldehyde type resin, urea and alkylated urea formaldehyde type resins, such'as the Lanaset manufactured by the American Cyanamid Company, Resloom manufactured by Monsanto, Rhonite manufactured by Rohm & Haas and the Beckamine manufactured bythe Reichold Chemical Corp. Many other common textile resins and finishing compounds may also prove satisfactory for this typeof treatment.

Examples of our process combining therein two steps, a partial chlorination and a resin treatment are given here below:

Example 1 A 100% wool flannel fabric, having a weight of 8 oz. per yard and consisting of 1/2'7s worsted yarn of 14 turns of S twist in the warp and 4% run woolen yarn of 15 turns of Z twist in the filling was wetted out in plain water and then immersed for approximately 90 seconds at room temperature in an acidified solution containing 0.05% free chlorine. Following this, the flannel was dechlorinated by a weak solution of sodium bisulfite and rinsed. It was then hydro-extracted and dried. The material was subsequently impregnated with a water emulsion containing 4% total solids of Durlana 3A resin. The excess emulsion was removed to an extent of 50% by passing the fabric through tight squeeze rolls thus leaving 2% of resin solids on the fabric. The flannel was then dried on a tenter frame.

The color, tensile strength and hand of the fabric was left almost unchanged by the treatment described. 7

The shrinkage results after 18 successive washings according to CCC-T-191A, Federal Specifications on washing are:

gfifi Flannel treated in shrglkage above manner- War'p Shrinkage, Warp Per cent Per cent 43. 1 3. 6

Example 2 A 100% wool fiannelfabric, having a weight of 8 oz. per yard and consisting of 1/275 worsted yarn of 14 turns of S twist in the warp and 4% run woolenyarn of 16 turns of Z twist inthe filling was wetted out with plain water and then immersed for approximately 90 seconds at room temperature in an acidified solution containing 0.09% free chlorine. Following this, the flannel was dechlorinated by a weak solution of sodium bisulfite, rinsed, hydro-extracted and dried. The material was then impregnated with a water emulsion containing 2% total solids of Koloc, the pH of the emulsion being between 2 and 3. Again, the excess of the emulsion was removed to an extent of 50% by passing the fabric through squeeze rolls thus leaving 1% of resin solids on the fabric. It was left'approximately r gggfi Flannel treated in Shrinkage above manner- Warp Shrinkage, Warp Per cent Per cent 47.1 3. IS

Example 3 A 100% wool material called robe flannel having a thread count of 15 TZT in the warp and 15 TZT in the filling and consisting of 4% run woolen yarn in the warp and 4% run woolen yarn in the filling was wetted out in plain water, immersed for approximately seconds at room temperature in an acidified solution containing 0.07 free chlorine. Following this the robe flannel was dechlorinated by a weak solution of sodium bisulfite and rinsed. It was then hydro-extracted and dried. The dry material was taken through a solution containing 8% total solids of Lanaset resin with auxiliary chemicals required for this resin and supplied by American Cyanamid Company. Again the excess of solution was removed to an extent of 50% by passing the fabric through squeeze rolls thus leaving 4% of resin solids 0n the fabric. The robe flannel was then dried on tenter frame without delay and cured for six minutes at a temperature of 280 degrees F. A subsequent rinsing bath containing a softener (Softener H made by American Cyanamid Co.) was then applied to improve the hand of the fabric.

The shrinkage caused after 18 successive washings according to CCC-T-l.91A by washing is as follows:

tgfgg i Flannel treated in shrinkaue above manner Warpa Shrinkage, Warp Per cent Per cent 41. 6 3. 1

Example 4 A wool material commonly called crepe, having a weight of 3 /2 oz. per yard and consisting of 1/35s worsted yarn of 1'7 turns of Z twist in the warp and of 1/52s worsted yarn of 14 turns of Z twist in the fillin was wetted out in plain water and then immersed for approxiinately 90 seconds at room. temperature in an acidified solution containing 0.03% free chlorine. Following this, the crepe material Was dechlorinated by a weak solution of sodium bisulfite, rinsed, hydro-extracted and dried. This time, it was impregnated with a solution containing 10% solids of Rhonite 313 plus 0.4% ammonium chloride. By passing the fabric through tight squeeze rolls a pick up of 50% was effected, thus leaving 5% of resin solids on the fabric. The crepe material was dried without delay and cured for eight minutes at 290 degrees F.

A slight stiffness was overcome by rinsing and application of /3% of Sapamine KW on the weight of the material. Shrinkage of this ma- 7 teriar after 12'successive washings according to CCC'T191A by Washing is as follows:

Untreated 7 crepe shrinkage,

Warp

Crepe treated in Shrinkage, Warp a Per cent Per cent Product above mannerv 5 Difference in Shrinkage Be- Per cent Shrinkage tween Treated Reduction No. of and Untreated, Washes Per Cent Per cent Warp Shrinkage Flannel (1):

1. Untreated 2. Halogenated 3. Resin 4. Addition of 2 plus 3 5. Ap licants dual Treatment Flannel (2 1. Untreated.... 2. Halogenated. 3. Resin. 4. Addition of 2 plus 3 5. Applicants dual Treatment Flannel (3).

1. Untreated 2. Halogcnated 3. Resin 4. Addition of 2 plus I 5. Applicants dual Treatment... Crepe (4):

1. Untreated 2. Halogenated. 3. Resin 4. Addition of 2 plus 3 5. Applicants dual Treatmen Challis (5):

1. Untreated 2. Halogenated 3. Resin 4. Addition of 2 plus 3 5. Applicants dual Treatment Example 5v A 100% wool material called challis having a weight of 3 oz. per yard and consisting of 1/38s worsted yarn of 17 turns of Z twist in the warp and 1/52s worsted yarn of 14 turns of Z twist in the filling was wetted out in plain water, immersed for approximately 90 seconds at room temperature in an acidified solution containing a 0.04% chlorine. Following this the challis material was dechlorinated by a weak solution of sodium bisulfite, rinsed, hydro-extracted, and dried. The dry challis was immersed in a solution containing 10% Resloom with auxiliary chemicals as supplied by the manufacturer. The excess of solution was removed to an extent of 50% by passing the fabric through tight squeeze rolls thus leaving 5% of resin solids on the fabric and then dried without delay, followed by a curing for 6 minutes at 290 degrees F. A slight stiffness of the fabric was overcome by rinsing and padding with Softener H made by American Cyanamid Company.

The shrinkage caused after 12 washings 2.0- w

cording to CCC-T-191A by washing is as follows;

As respects a resin treatment, no satisfactory anti-felting of wool fabrics by treatment with resin alone can. be obtained, except by using substantially large quantities of resin upon the fabric. Using such high quantities of resin, the undesirable features concurrent with the resulting felt-proofing would by far out-weigh the subjective advantages obtained through the antifelting treatment with resin alone. On the other hand, when the resin treatment follows the halogenation process, it is. possible to obtain very satisfactory results with very small percentages of resin, whereby the disadvantageous qualities 0' inherent in a resin treatment alone are eliminated. As respects the chlorination treatment alone, no satisfactory anti-felting of wool fabrics by chlorination can be obtained as the amount of chlorine necessary to obtain non-felting properties will be deleterious to the generaland specific properties required of the finished textile material. Our process is not limited to application to pure wool fabrics alone, so that fabrics made of blends of wool with cotton and with other textile fibres can be satisfactorily treated in this manner. Neither step of our process is sufficiently drastic to harm the physical properties of the fabrics and the fibres.

Having thus described our invention, what we desire to secure by Letters Patent is as follows:

1. A process for the anti-felting of wool and wool products which comprises as steps first treating the material by a partial halogenation and thereafter subjecting the partially halogenated 75 material to a resin treatment. the successive treatments being each incapable by itself to produce effective non-felting properties.

2. A process for the anti-felting of wool and wool products which comprises a, preliminary wettingpf the material, thereafter immersing the wetted material in a bath containing 0.03% to 0.09% free acidified ions of the group comprising chlorine and bromine, thereafter dehalogenating the material by immersion in a weak solution of sodium bisulphite, and impregnating the materials with a resin in solution, which resin treatment in itself is insumcient except when preceded by a partial halogenation treatment to produce satisfactory non-felting properties.

3. The process according to claim 1 for the anti-felting of wool and wool, products which coniprises the treating of the material by a partial halogenation, and thereafter impregnating the partially halogenated material with resins of the group of polymerized diolefines in aqueous solutions, which resin treatment in itself is insufficient except when it is preceded by a partial halogenation treatment to produce satisfactory nonfelting properties.

4. The process according to claim 1 for the antifelting of wool and wool products which comprises the treating of the material by a partial halogenation, and thereafter impregnating the partially halogenated material with resins of the group of alkylated melamine formaldehyde resins in aqueous solutions, which resin treatment in itself is insufficient except when it is preceded by a partial halogenation treatment to produce satisfactory non-felting properties.

5. The process according to claim 1 for the anti-felting of wool and wool products which comprises the treating of the material by a partial halogenation, and thereafter impregnating the partiall halogenated material with resins of the group of urea and alkylated urea formaldehyde resins in aqueous solutions, which resin treatment in itself is insufficient except when it is preceded by a partial halogenation treatment to produce satisfactory non-felting properties.

6. The process according to claim 1 for the anti-felting of wool and wool products which comprises the treating of the material by a partial halogenation and thereafter impregnating the partially halogenated. material with a water emulsion containing 4% total solids polymerized diolefines, thereafter removing the excess emulsion by passing the material through tight squeeze rolls, the resin treatment in itself being insufficient except when preceded by a partial halogenation treatment to produce satisfactory non-felting properties.

'7. The process according to claim 1 for the anti-felting of wool and wool products which comprises the treating of the material by a partial halogenation and thereafter impregnating the partially halogenated material with a Water emulsion containing 2% total solids of polymerized diolefines thereafter removing the excess emulsion, the resin treatment in itself being insufilcient 10 except when preceded by a partial halogenation treatment to produce satisfactor non-felting properties.

8. The process according to claim 1 for the anti-felting of wool and wool products which comprises the treating of the material by a partial halogenation and thereafter impregnating the partially halogenated material with a 'water emulsion containing 10% total solids, comprising ureaformaldehyde type resin and 0.4% ammonium chloride, thereafter removing the excess emulsion by passing the material through tight squeeze rolls, thereafter drying and curing the material, the cured material being rinsed and treating the rinsed material with of a softener, the resin treatment in itself being insufficient except when preceded by a partial halogenation treatment to produce satisfactory non-felting properties.

9. The process according to claim 1 for the anti-felting of wool and wool products which comprises the treating of the material by a partial halogenation and thereafter impregnating the partially halogenated material with a-water emu1- sion containing 10% total solids, comprising methylol-melamine resin, a methylated melamine formaldehyde resin, and 0.4% ammonium chloride, thereafter removing the excess emulsion by passing the material through tight squeeze rolls, thereafter drying and curing the material, the cured material being rinsed and treating the rinsed material with of a softener, the resin treatment in itself being insufficient except when preceded by a partial halogenation treatment to produce satisfactory non-felting properties.

0. The process according to claim 1 for the anti-felting of wool and wool products which comprises the treating of the material by a partial halogenation and thereafter impregnating the partially halogenated material with a water emulsion containing 10% total solids, comprising a methylol-melamine condensation product treated with methyl alcohol and 0.4% ammonium chloride, thereafter removing the excess emulsion by passing the material through tight squeeze rolls, thereafter drying and curing the material, the cured material being rinsed and treating the rinsed material with of a softener, the resin. treatment in itself being insufficient except when preceded by a partial halogenation treatment to produce satisfactory non-felting properties.

FREDERICK R. I-IAIGH. HUGO EHRHARDT. ERNEST C. KOERNER.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS- Number Name Date 2,383,963 Gottfried Sept. 4, 1945 2,395,724 Cowley Feb. 26, 1946 2,395,791 Pfefier Feb. 26, 1946 

1. A PROCESS FOR THE ANTI-FELTING OF WOOL AND WOOL PRODUCTS WHICH COMPRISES AS STEPS FIRST TREATING THE MATERIAL BY A PARTIAL HALOGENATION AND THEREAFTER SUBJECTING THE PARTIALLY HALOGENATED MATERIAL TO A RESIN TREATMENT, THE SUCCESSIVE TREATMENTS BEING EACH INCAPABLE BY ITSELF TO PRODUCE EFFECTIVE NON-FELTING PROPERTIES. 